CN101940918B - Method for treating magnesium silicate adsorbent - Google Patents
Method for treating magnesium silicate adsorbent Download PDFInfo
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- CN101940918B CN101940918B CN200910012485.5A CN200910012485A CN101940918B CN 101940918 B CN101940918 B CN 101940918B CN 200910012485 A CN200910012485 A CN 200910012485A CN 101940918 B CN101940918 B CN 101940918B
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Abstract
The invention discloses a method for treating a magnesium silicate adsorbent. The method comprises the following steps of: removing water of the magnesium silicate adsorbent; dipping with alcohol with 1 to 4 carbon atoms; and finally, drying and roasting. The method for treating the magnesium silicate adsorbent is characterized in that: (1) the magnesium silicate is dipped with an organic solvent so as to eliminate the difference of the property of the magnesium silicate adsorbent caused by impurity adsorption and improve the adsorption stability and repeatability of the magnesium silicate adsorbent; (2) the magnesium silicate is activated, wherein the magnesium silicate has higher adsorption efficiency for polar substances in the activated state, and has higher reclaiming rate for non-polar substances (petroleum type); and (3) the activation treatment process is shorter than the deactivation treatment process so as to save mass time. The method is particularly suitable for treating the magnesium silicate adsorbent used for petroleum hydrocarbon analysis, and can effectively adsorb polar non hydrocarbon organics in the extract of water, soil or solid waste samples and eliminate the interference thereof on petroleum hydrocarbon determination.
Description
Technical field
The present invention relates to a kind of processing method of magnesium silicate adsorbent, the processing method of the magnesium silicate adsorbent that particularly water quality petroleum class and vegetable and animals oils are used in measuring.The magnesium silicate adsorbent of processing of the present invention can effectively adsorb and eliminate the interference that water, soil or solid waste sample extraction liquid Semi-polarity nonhydrocarbon organic matter are measured petroleum hydrocarbon.
Background technology
Oily substance is the problem of global concern to the pollution of water body, the water that polluted by petroleum-type has oily taste, toxic to biology, the water surface can form oil film, destroy its dissolved oxygen balance, concerning water environment, oily substance is a kind of major pollutants, and wherein petroleum substance is the most outstanding organic pollution.Therefore the degree of accuracy that, water quality petroleum class is measured is most important to environmental monitoring, assessment and improvement.
At present, the standard method that China measures water quality petroleum class is " the mensuration infrared spectrophotometry of GB/T 16488-1996 water-quality petroleum and vegetable and animals oils ", the processing procedure of the magnesium silicate adsorbent that wherein used is: get 60～100 order magnesium silicates in porcelain evaporating dishes, be placed in 500 DEG C of heating 2h in high temperature furnace, be chilled to approximately 200 DEG C in stove after, move in drier and be chilled to room temperature, in ground glass stoppered bottle, preserve.When use, take appropriate dry magnesium silicate and be placed in ground glass stoppered bottle, according to the weight of dry magnesium silicate, add appropriate distilled water carry out deactivation in the ratio of 6% (m/m), Mi Sai also fully vibrates several minutes, uses after placing about 12h.
Due to the difference of production and laboratory environment, the pollution bringing in magnesium silicate preparation and put procedure is different, and this will directly affect repeatability and the accuracy of petroleum substance measurement result.Magnesium silicate needs the time of placement longer in deactivation process, and the magnesium silicate after deactivation weakens greatly to the adsorption efficiency of water quality Semi-polarity material, cause the measurement result of petroleum-type higher, thereby affected the accuracy of environment measuring and assessment, brought inconvenience to environmental improvement.
Summary of the invention
For the deficiency of existing magnesium silicate adsorbent processing procedure, the invention provides the processing method that uses magnesium silicate adsorbent in a kind of water quality petroleum class and vegetable and animals oils mensuration process, it is reproducible that the magnesium silicate adsorbent of the inventive method processing has measurement result, to the absorption efficiency advantages of higher of polar substances.
The processing method process of magnesium silicate adsorbent of the present invention is as follows: first remove the water of adsorption of magnesium silicate, then adopt the alcohol dipping of C1～C4, be finally dried and calcination process.
In the processing method of magnesium silicate adsorbent of the present invention, the method for operating that removes adsorption of magnesium silicate water is low-temperature bake method, as can be at 100～140 DEG C roasting 2～6h.
In the processing method of magnesium silicate adsorbent of the present invention, the magnesium silicate after dehydration adopts the alcohol dipping of C1～C4, and dipping can adopt saturated dipping, also can adopt supersaturation dipping, and dipping temperature is to use below the boiling temperature of alcohol, and dip time is 10～60 minutes.Particular methanol, ethanol, normal propyl alcohol, isopropyl alcohol etc. in the alcohol of C1～C4.The alcohol dipping of C1～C4 can adopt dry mode that alcohol is removed later, is dried and can adopts constant pressure and dry or vacuum drying, and dry temperature is generally 20～200 DEG C, is generally 1～5 hour drying time.Dried calcination process condition is roasting 1～5 hour at 450～550 DEG C.While being cooled to 100～250 DEG C after roasting, put into drier cooling down.
In the processing method of magnesium silicate adsorbent of the present invention, key is that (1) with an organic solvent carry out impregnation process to magnesium silicate, can eliminate so the qualitative difference of magnesium silicate adsorbent that different production and environment for use are brought, improve absorption stability and the repeatability of magnesium silicate adsorbent.(2) magnesium silicate adopts activation method.Under the state of activation, magnesium silicate is higher to the adsorption efficiency of polar substances, and also higher to the rate of recovery of apolar substance (petroleum-type).(3) activation processing process is shorter than the deactivation processing procedure time, has saved a large amount of time.
In the processing method of magnesium silicate adsorbent of the present invention, stability and repeatability through the magnesium silicate after organic solvent dipping to measurement result are greatly improved, and magnesium silicate after activation also improves greatly to the absorption efficiency of polar substances.Experiment shows, can reach < 0.3% to the relative standard deviation of measuring petroleum-type, can reach < 0.5% to the relative standard deviation of measuring polar substances.And the magnesium silicate not soaking through alcohols material is 1.36%～14.6% to the relative standard deviation of petroleum-type, be 1.07%～7.80% to the relative standard deviation of polar substances; Magnesium silicate after activated can reach 99.7%～103% to the rate of recovery of petroleum-type, can reach 99.1%～100% to the adsorption efficiency of polar substances.Magnesium silicate after deactivation can reach 97.6%～99.5% to the rate of recovery of petroleum-type, and the adsorption efficiency of polar substances is only had to 51.3%～53.5%.
Brief description of the drawings
Fig. 1 is the glass chromatography column schematic diagram that magnesium silicate is housed.
In figure: 1-magnesium silicate adsorbent, 2-mineral wool, 3-glass chromatography column.
Detailed description of the invention
A kind of concrete operation step of the processing method of magnesium silicate adsorbent of the present invention is as follows:
(1) get 60～100 order magnesium silicates in porcelain evaporating dishes, 100～140 DEG C of dry 2～6h of low temperature, remove physical absorption water.
(2) magnesium silicate after dehydration is flooded with the alcohol of C1～C4, its volume ratio is: V
alcohol: V
silicic acid magnesium=2: 1～3: 1, dip time is preferably 30～50min.
(3) be put in the drier vacuumizing after the magnesium silicate having flooded is drained and carry out drying at room temperature, be preferably 2～4h drying time.
(4) dried magnesium silicate is carried out to high-temperature roasting, temperature is 450～550 DEG C, and the time is preferably 2～3h.
(5) magnesium silicate roasting moves in drier and is chilled to room temperature after being chilled to approximately 200 DEG C after completing in stove, in ground glass stoppered bottle, preserves, stand-by.
By above-mentioned magnesium silicate load map 1 glass chromatography column of handling well (
) in, magnesium silicate packed height is 80mm, a small amount of mineral wool is clogged in glass chromatography column exit.
The light diesel fuel (200～350 DEG C of boiling range scopes) that nonpolar standard sample selects Russian imported crude oil straight run to go out.The above-mentioned light diesel fuel of 5 same concentrations of preparation, respectively by above-mentioned magnesium silicate glass chromatographic column, then measures the light diesel fuel after absorption they respectively by chromatography, verifies the repeatability of magnesium silicate to apolar substance absorption by measurement result.
Polarity standard's sample is selected methyl hexadecanoate.The methyl hexadecanoate of 5 same concentrations of preparation, respectively by above-mentioned magnesium silicate glass chromatographic column, then measures the methyl hexadecanoate after absorption they respectively by chromatography, verifies the repeatability of magnesium silicate to polar substances absorption by measurement result.
The nonpolar standard sample of 3 variable concentrations of preparation, by them respectively by above-mentioned magnesium silicate glass chromatographic column, then the light diesel fuel after absorption is measured respectively by chromatography, verified the rate of recovery of magnesium silicate to variable concentrations apolar substance by measurement result.
Polarity standard's sample of 3 variable concentrations of preparation, by them respectively by above-mentioned magnesium silicate glass chromatographic column, then the methyl hexadecanoate after absorption is measured respectively by chromatography, verified the absorption efficiency of magnesium silicate to variable concentrations polar substances by measurement result.
Chromatographic condition: 280 DEG C of injector temperatures, 300 DEG C of detector temperatures, 45 DEG C of column temperatures (3min), rise to 280 DEG C (30min) with 12 DEG C/min, flow rate of carrier gas 1.5mL/min, Splitless injecting samples (not shunting time 0.75min), hydrogen flow rate 35mL/min, air velocity 400mL/min, sample size 1 μ L.
Set forth technical scheme of the present invention below in conjunction with embodiment, but be not limited to the embodiment of the present invention.
Embodiment 1
(1) get 50g 60～100 order magnesium silicates in porcelain evaporating dishes, 140 DEG C of dry 4h of low temperature, remove physical absorption water.
(2) magnesium silicate is carried out to saturated immersion with ethanol, its volume ratio is: V
ethanol: V
magnesium silicate=2: 1, dip time is 40min.
(3) magnesium silicate having flooded is put in the drier vacuumizing and carries out drying at room temperature, be 2h drying time.
(4) dried magnesium silicate is carried out to high-temperature roasting, temperature is 500 DEG C, and the time is 3h.
(5) magnesium silicate roasting moves in drier and is chilled to room temperature after being chilled to approximately 200 DEG C after completing in stove, in ground glass stoppered bottle, preserves, stand-by.
(6) above-mentioned magnesium silicate after treatment is slowly poured in Fig. 1 glass chromatography column, limit bevelling beats gently, and the packed height of magnesium silicate is 80mm.A small amount of mineral wool is clogged in glass chromatography column exit.
(7) weigh 0.0750g nonpolar standard sample, be settled to 50mL with carrene, it is 1.5 × 10 that same method makes 5 concentration altogether
3the light diesel fuel of ng/ μ L.They are crossed respectively to above-mentioned magnesium silicate glass chromatographic column, filtrate is settled to respectively to 100mL with carrene.
Diesel oil after adsorption of magnesium silicate is measured respectively by chromatography, and repeatability the results are shown in Table 1.
Table 1 adsorption of magnesium silicate diesel oil repeatability
(8) weigh 0.1002g polarity standard sample, be settled to 50mL with carrene, it is 2.00 × 10 that same method is prepared 5 concentration altogether
3the polarity standard specimen methyl hexadecanoate of ng/ μ L.They are crossed respectively to above-mentioned magnesium silicate glass chromatographic column, filtrate is settled to respectively to 100mL with carrene.
Methyl hexadecanoate after adsorption of magnesium silicate is measured respectively by chromatography, and repeatability the results are shown in Table 2.
Table 2 is methyl hexadecanoate concentration repeatability after absorption
(9) weigh respectively 0.1001g, 0.2004g, the nonpolar standard sample of 0.3011g, be settled to respectively 50mL with carrene, be mixed with 3 variable concentrations light diesel fuels.They are crossed respectively to above-mentioned magnesium silicate glass chromatographic column, filtrate is settled to respectively to 100mL with carrene.
After adsorption of magnesium silicate, diesel oil is measured respectively by chromatography, and the rate of recovery the results are shown in Table 3.
The rate of recovery of table 3 to variable concentrations light diesel fuel
| Concentration before absorption, ng/ μ L | Concentration after absorption, ng/ μ L | The rate of recovery, % |
| 2.00×10 3 | 1.03×10 3 | 103 |
| 4.01×10 3 | 2.00×10 3 | 99.8 |
| 6.02×10 3 | 3.00×10 3 | 99.7 |
(10) weigh respectively 0.0512g, 0.1002g, 0.2015g polarity standard sample, be settled to respectively 50mL with carrene, be mixed with the polarity standard specimen methyl hexadecanoate of 3 variable concentrations.They are crossed respectively to above-mentioned magnesium silicate glass chromatographic column, filtrate is settled to respectively to 100mL with carrene.
After adsorption of magnesium silicate, methyl hexadecanoate is measured respectively by chromatography, and absorption efficiency the results are shown in Table 4.
The absorption efficiency of table 4 to variable concentrations polarity standard specimen methyl hexadecanoate
| Concentration before absorption, ng/ μ L | Concentration after absorption, ng/ μ L | Absorption efficiency, % |
| 1.02×10 3 | 0.70 | 99.9 |
| 2.00×10 3 | 2.02 | 99.8 |
| 4.03×10 3 | 12.1 | 99.4 |
Embodiment 2
(1) get 50g 60～100 order magnesium silicates in porcelain evaporating dishes, 130 DEG C of dry 2h of low temperature, remove physical absorption water.
(2) magnesium silicate after dehydration is carried out to saturated immersion, V with isopropyl alcohol
isopropyl alcohol: V
magnesium silicate=3: 1.Soak time is 50min.
(3) magnesium silicate having flooded is put in the drier vacuumizing and is dried at 80 DEG C, be 3h drying time.
(4) dried magnesium silicate is carried out to high-temperature roasting, temperature is 500 DEG C, and the time is 2.5h.
(5) magnesium silicate roasting moves in drier and is chilled to room temperature after being chilled to approximately 200 DEG C after completing in stove, in ground glass stoppered bottle, preserves, stand-by.
(6) above-mentioned magnesium silicate after treatment is slowly poured in Fig. 1 glass chromatography column, limit bevelling beats gently, and the packed height of magnesium silicate is 80mm.A small amount of mineral wool is clogged in glass chromatography column exit.
(7) weigh 0.1502g nonpolar standard sample, be settled to 50mL with carrene, it is 3.0 × 10 that same method makes 5 concentration altogether
3the light diesel fuel of ng/ μ L.They are crossed respectively to above-mentioned magnesium silicate glass chromatographic column, filtrate is settled to respectively to 100mL with carrene.
Diesel oil after adsorption of magnesium silicate is measured respectively by chromatography, and repeatability the results are shown in Table 5.
Table 5 is diesel oil concentration repeatability after absorption
(8) weigh 0.1501g polarity standard sample, be settled to 50mL with carrene, it is 3.00 × 10 that same method is prepared 5 concentration altogether
3the polarity standard specimen methyl hexadecanoate of ng/ μ L.They are crossed respectively to above-mentioned magnesium silicate glass chromatographic column, filtrate is settled to respectively to 100mL with carrene.
Methyl hexadecanoate after adsorption of magnesium silicate is measured respectively by chromatography, and repeatability the results are shown in Table 6.
Table 6 is methyl hexadecanoate concentration repeatability after absorption
(9) weigh respectively 0.0831g, 0.1526g, the nonpolar standard sample of 0.2504g, be settled to respectively 50mL with carrene, be mixed with 3 variable concentrations light diesel fuels.They are crossed respectively to above-mentioned magnesium silicate glass chromatographic column, filtrate is settled to respectively to 100mL with carrene.
After adsorption of magnesium silicate, diesel oil is measured respectively by chromatography, and the rate of recovery the results are shown in Table 7.
The rate of recovery of table 7 to variable concentrations light diesel fuel
| Concentration before absorption, ng/ μ L | Concentration after absorption, ng/ μ L | The rate of recovery, % |
| 1.66×10 3 | 832 | 100 |
| 3.05×10 3 | 1.53×10 3 | 100 |
| 5.01×10 3 | 2.50×10 3 | 99.8 |
(10) weigh respectively 0.1534g, 0.2506g, 0.3123g polarity standard sample, be settled to respectively 50mL with carrene, be mixed with the polarity standard specimen methyl hexadecanoate of 3 variable concentrations.They are crossed respectively to above-mentioned magnesium silicate glass chromatographic column, filtrate is settled to respectively to 100mL with carrene.
After adsorption of magnesium silicate, methyl hexadecanoate is measured respectively by chromatography, and absorption efficiency the results are shown in Table 8.
The absorption efficiency of table 8 to variable concentrations polarity standard specimen methyl hexadecanoate
| Concentration before absorption, ng/ μ L | Concentration after absorption, ng/ μ L | Absorption efficiency, % |
| 3.07×10 3 | 7.67 | 99.5 |
| 5.01×10 3 | 20.4 | 99.2 |
| 6.25×10 3 | 24.9 | 99.2 |
Claims (9)
1. a processing method for magnesium silicate adsorbent, is characterized in that: first remove the water of adsorption of magnesium silicate, then adopt the alcohol dipping of C1～C4, be finally dried and calcination process; Dried calcination process condition is roasting 1～5 hour at 450～550 DEG C.
2. in accordance with the method for claim 1, it is characterized in that: the method for operating that removes adsorption of magnesium silicate water is low-temperature bake method roasting 2～6h at 100～140 DEG C.
3. in accordance with the method for claim 1, it is characterized in that: described C1～C4 alcohol dipping adopts saturated dipping, or adopt supersaturation dipping.
4. according to the method described in claim 1 or 3, it is characterized in that: dipping temperature is to use below the boiling temperature of alcohol, and dip time is 10～60 minutes.
5. according to the method described in claim 1 or 3, it is characterized in that: the alcohol of C1～C4 is methyl alcohol, ethanol, normal propyl alcohol or isopropyl alcohol.
6. it is characterized in that in accordance with the method for claim 1: dry employing constant pressure and dry or vacuum drying after alcohol dipping.
7. according to the method described in claim 1 or 6, it is characterized in that: dry temperature is 20～200 DEG C, be 1～5 hour drying time.
8. in accordance with the method for claim 1, it is characterized in that: while being cooled to 100～250 DEG C after magnesium silicate roasting, put into drier cooling down.
9. it is characterized in that in accordance with the method for claim 1: when dipping, the volume ratio of alcohol and magnesium silicate is 2: 1～3: 1.
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| CN1343204A (en) * | 1999-03-16 | 2002-04-03 | 国际壳牌研究有限公司 | Process for purification of propylene oxide |
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| CN1343204A (en) * | 1999-03-16 | 2002-04-03 | 国际壳牌研究有限公司 | Process for purification of propylene oxide |
Non-Patent Citations (1)
| Title |
|---|
| 夏晓萍等.红外光谱法测定城市污泥中油类的方法探讨.《市政技术》.2008,第26卷(第3期),第219页左栏第8-10行. * |
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